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NASA NTRS1994

Innovative instrumentation for mineralogical and elemental analyses of solid extraterrestrial surfaces: The Backscatter Moessbauer Spectrometer/X Ray Fluorescence analyzer (BaMS/XRF)

We have developed a four-detector research-grade backscatter Moessbauer spectrometer (BaMS) instrument with low resolution x-ray fluorescence analysis (XRF) capability. A flight-qualified instrument based on this design would be suitable for use on missions to the surfaces of solid solar-system objects (Moon, Mars, asteroids, etc.). Target specifications for the flight instrument are as follows: mass less than 500 g; volumes less than 300 cu cm; and power less than 2 W. The BaMS/XRF instrument would provide data on the oxidation state of iron and its distribution among iron-bearing mineralogies and elemental composition information. This data is a primary concern for the characterization of extraterrestrial surface materials.

Shelfer, T. D.↗

NASA NTRS2003

Astrobiological Significance of Chemolithoautotrophic Acidophiles

For more than a century (since Winogradsky discovered lithoautotrophic bacteria) a dilemma in microbiology has concerned life that first inhabited the Earth. Which types of life forms first appeared in the primordial oceans during the earliest geological period on Earth as the primary ancestors of modem biological diversity? How did a metabolism of ancestors evolve: from lithoautotrophic to lithohetherotrophic and organoheterotrophic or from organoheterotrophic to organoautotrophic and lithomixotrophic types? At the present time, it is known that chemolithoheterotrophic and chemolithoautotrophic metabolizing bacteria are wide spread in different ecosystems. On Earth the acidic ecosystems are associated with geysers, volcanic fumaroles, hot springs, deep sea hydrothermal vents, caves, acid mine drainage and other technogenic ecosystems. Bioleaching played a significant role on a global geological scale during the Earth's formation. This important feature of bacteria has been successfully applied in industry. The lithoautotrophs include Bacteria and Archaea belonging to diverse genera containing thermophilic and mesophilic species. In this paper we discuss the lithotrophic microbial acidophiles and present some data with a description of new acidophilic iron- and sulfur- oxidizing bacterium isolated from the Chena Hot Springs in Alaska. We also consider the possible relevance of microbial acidophiles to Venus, Io, and acidic inclusions in glaciers and icy moons.

Pikuta, Elena V.↗

NASA NTRS2005

RIO Tinto Faulted Volcanosedimentary Deposits as Analog Habitats for Extant Subsurface Biospheres on Mars: A Synthesis of the MARTE Drilling Project Geobiology Results

Geochemistry and mineralogy on Mars surface characterized by the MER Opportunity Rover suggest that early Mars hosted acidic environments in the Meridiani Planum region [1, 2]. Such extreme paleoenvironments have been suggested to be a regional expression of the global Mars geological cycle that induced acidic conditions by sulfur complexation and iron buffering of aqueous solutions [3]. Under these assumptions, underground reservoirs of acidic brines and, thereby, putative acidic cryptobiospheres, may be expected. The MARTE project [4, 5] has performed a drilling campaign to search for acidic and anaerobic biospheres in R o Tinto basement [6] that may be analogs of these hypothetical communities occurring in cryptic habitats of Mars. This Rio Tinto geological region is characterized by the occurrence of huge metallic deposits of iron sulfides [7]. Late intensive diagenesis of rocks driven by a compressive regimen [8] largely reduced the porosity of rocks and induced a cortical thickening through thrusting and inverse faulting and folding. Such structures play an essential role in transporting and storing water underground as any other aquifers do in the Earth. Once the underground water reservoirs of the Ro Tinto basement contact the hydrothermal pyrite deposits, acidic brines are produced by the release of sulfates and iron through the oxidation of sulfides [9].

Fernandez-Remolar, D. C.↗

NASA NTRS2006

Characterization and Petrologic Interpretation of Olivine-Rich Basalts at Gusev Crater, Mars

Rocks on the floor of Gusev crater are basalts of uniform composition and mineralogy. Olivine, the only mineral to have been identified or inferred from data by all instruments on the Spirit rover, is especially abundant in these rocks. These picritic basalts are similar in many respects to certain Martian meteorites (olivine-phyric shergottites). The olivine megacrysts in both have intermediate compositions, with modal abundances ranging up to 20-30%. Associated minerals in both include low-calcium and high-calcium pyroxenes, plagioclase of intermediate composition, iron-titanium-chromium oxides, and phosphate. These rocks also share minor element trends, reflected in their nickel-magnesium and chromium-magnesium ratios. Gusev basalts and shergottites appear to have formed from primitive magmas produced by melting an undepleted mantle at depth and erupted without significant fractionation. However, apparent differences between Gusev rocks and shergottites in their ages, plagioclase abundances, and volatile contents preclude direct correlation. Orbital determinations of global olivine distribution and compositions by thermal emission spectroscopy suggest that olivine-rich rocks may be widespread. Because weathering under acidic conditions preferentially attacks olivine and disguises such rocks beneath alteration rinds, picritic basalts formed from primitive magmas may even be a common component of the Martian crust formed during ancient and recent times.

McSween, H. Y.↗

NASA NTRS2004

Precipitation of Secondary Phases from the Dissolution of Silicate Glasses

Basaltic and anorthositic glasses were subjected to aqueous weathering conditions in the laboratory where the variables were pH, temperature, glass composition, solution composition, and time. Leached layers formed at the surfaces of glasses followed by the precipitation of X-ray amorphous iron and titanium oxides in acidic and neutral solutions at 25 C over time. Glass under oxidative hydrothermal treatments at 150 C yielded a three-layered surface; which included an outer smectite layer, a Fe-Ti oxide layer and an innermost thin leached layer. The introduction of Mg into solutions facilitated the formation of phyllosilicates. Aqueous hydrothermal treatment of anorthositic glasses (high Ca, low Ti) at 200 C readily formed smectite, whereas, the basaltic glasses (high Ti) were more resistant to alteration and smectite was not observed. Alkaline hydrothermal treatment at 2000e produced zeolites and smectites; only smectites formed at 200 C in neutral solutions. These mineralogical changes, although observed under controlled conditions, have direct applications in interpreting planetary (e.g., meteorite parent bodies) and terrestrial aqueous alteration processes.

Ming, Douglas W.↗

NASA NTRS2014

Coordinated Mineralogical and Isotopic Analysis of a Cosmic Symplectite Identified in a Stardust Terminal Particle

Comet Wild-2 samples returned by the Stardust spacecraft contain a chemically diverse mixture of material, underscoring the complex nature of comets. Studies of entire Stardust aerogel tracks afford the opportunity to examine the fine-grained particle fragments distributed along the length of the track as well as the terminal particles. Previous TEM characterization of a terminal particle (TP) in track #147 revealed a symplectically intergrown iron sulfide and oxide assemblage. Mineralogically similar assemblages, known as cosmic symplectites (COS, formerly termed "new-PCP"), have only been identified in the primitive carbonaceous chondrite Acfer 094. Meteoritic COS have isotopically heavy O compositions (delta (sup 17), O-18 = 180per mille) that point to interactions with early solar system primordial water. In this study we report mineralogical and O isotopic measurements of the Wild-2 COS assemblage. Experimental: Track #147 is a "bulbous"-type track (4600 microns long) containing 7 terminal particles. The TPs were removed from the track, embedded in epoxy, and ultramicrotomed. A JEOL 2500SE 200 keV field-emission scanning-transmission electron microscope was used to obtain quantitative elemental maps and detailed mineralogical characterization. Following TEM analysis, two thin sections of TP4 (12 microns) were analyzed for O isotopes by raster ion imaging with the JSC NanoSIMS 50L. All three O isotopes were measured simultaneously using electron multipliers. San Carlos olivine grains were used as isotopic standards. Results and Discussion: The COS in the Wild-2 track #147 TP4 sample consists of symplectically intergrown pentlandite and nanocrystalline maghemite which coexists with high-Ca pyroxene with Na and Cr (kosmochlor component). This kosmochlor component could have a nebular origin and be precursors to type II chondrules in ordinary chondrites. Yet pentlandite is not a stable phase in the nebula. The COS in Acfer 094 also consists of pentlandite, but contains magnetite [4] rather than the more oxidized maghemite observed in the Wild-2 COS. The Acfer 094 COS display heavy O isotopic compositions that are the result of sulfidization and oxidation of Fe, Ni-metal grains and sulfides by O-17- and O-18-rich water in the solar nebula or possibly on the parent body. The O isotopic composition of the Wild-2 COS, however, is indistinguishable from terrestrial, indicating it was not altered by the same primordial aqueous reservoir as the Acfer 094 COS. The alteration could have occurred on the parent body by isotopically equilibrated ice. The mineralogy and petrography of Wild-2 samples suggests an incomplete or nascent hydration process. In future work we will analyze S isotopes in the track #147 TP4 COS and search for additional COS in Stardust samples.

Nguyen, A. N.↗

NASA NTRS2020

X-ray Amorphous Components of Antarctica Dry Valley Soils: Weathering Implications for Mars

The Antarctic Dry Valleys (ADV) comprise the largest ice-free region of Antarctica. Precipitation usually occurs as snow, relative humidity is frequently low, and mean annual temperatures are about -20°C [1]. Substantial work has focused on soil formation in the ADVs [2], however, little work has focused on the mineralogy of secondary alteration phases. The dominant weathering process in the ADV region is physical weathering, however, chemical weathering has been well documented [3]. The occurrence of chemical weathering processes are suggested by the presence of clay minerals and iron and titanium oxides in soil. Previously we have investigated soils from two sites in the ADV’s and have shown evidence of chemical weathering by the presence of clay minerals (vermiculite, smectite), short-range ordered (SRO) and/or X-ray amorphous materials, and Fe- and Tioxides as well as the presence of discrete calcite crystals [4, 5]. The Chemistry and Mineralogy (CheMin) instrument onboard the Mars Curiosity rover has detected abundant amounts (approx. 25-30 wt. %) of X-ray amorphous materials in a windblown deposit or “soil” (Rocknest) and in a sedimentary rocks [6,7,8]. The occurrence of large amounts of X-ray amorphous materials in Mars sediments is surprising because these materials are usually present in small quantities in terrestrial environments. The objective of this study is to further characterize the chemistry and mineralogy, specifically the secondary alteration mineralogy and the presence of X-ray amorphous material, of soils from two sites we have previously studied, a subxerous soil in Taylor Valley, and an ultraxerous soil in University Valley. While the chemical alteration processes and mineralogy of the ADV has been documented previously, there has been limited discussion on the occurrence and formation of X-ray amorphous and SRO materials in Antarctica soils. The process of aqueous alteration in the ADVs may have implications for pedogenic processes on Mars, and may lead to a better understanding to the abundance of amorphous material found in sediments in Gale crater.

Quinn, J. E.↗

NASA NTRS2022

Geological, Multispectral, and Meteorological Imaging Results from the Mars 2020 Perseverance Rover in Jezero Crater

Perseverance’s Mastcam-Z instrument provides high-resolution stereo and multispectral images with a unique combination of spatial resolution, spatial coverage, and wavelength coverage along the rover’s traverse in Jezero crater, Mars. Images reveal rocks consistent with an igneous (including volcanic and/or volcaniclastic) and/or impactite origin and limited aqueous alteration, including polygonally fractured rocks with weathered coatings; massive boulder-forming bedrock consisting of mafic silicates, ferric oxides, and/or iron-bearing alteration minerals; and coarsely layered outcrops dominated by olivine. Pyroxene dominates the iron-bearing mineralogy in the fine-grained regolith, while olivine dominates the coarse-grained regolith. Solar and atmospheric imaging observations show significant intra- and intersol variations in dust optical depth and water ice clouds, as well as unique examples of boundary layer vortex action from both natural (dust devil) and Ingenuity helicopter–induced dust lifting. High-resolution stereo imaging also provides geologic context for rover operations, other instrument observations, and sample selection, characterization, and confirmation.

Mars 2020↗

NASA NTRS1968

Secondary iron-air batteries

Self discharge, capacity maintenance, oxidation, and water loss problems in secondary iron-air batteries

Wagner, O. C.↗

DOE OSTI2024

Enhancing nitrogen fixation efficiency in glow-like discharge by reducing cathode-fall voltage

In plasma nitrogen fixation devices, discharge electrodes are crucial yet susceptible to oxidation and corrosion due to plasma’s high temperatures and oxygen content, which could alter discharge modes. This research evaluates the impact of different electrode materials, including iron, chromium, nickel, copper, and 304 stainless steel, on nitrogen fixation efficiency in glow-like discharges driven by high-voltage DC power. Notably, iron and 304 stainless steel cathodes undergo a mode transition at increased currents, evident from plasma color shifts and significant voltage reductions. Fourier transform infrared spectroscopy analyses reveal that such mode changes minimally affect nitrogen oxide production rates, leading to a notable decrease in energy consumption for nitrogen fixation by up to 40%. OES and SEM-EDS measurements suggest that iron oxide, with its higher secondary electron emission, replaces metal as the cathode material, facilitating mode transitions and maintaining discharge current at lower voltages. Further, this voltage change is largely attributed to the cathode voltage drop, highlighting the minimal role of the cathode fall region in NO x synthesis. These findings underscore the potential for improving plasma nitrogen fixation energy efficiency by choosing suitable cathode materials to lower the cathode-fall voltage.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2022

Probing the initial stages of iron surface corrosion: Effect of O 2 and H 2 O on surface carbonation

Iron plays a vital role in natural processes such as water, mineral, iron, and nutrient cycles. Iron undergoes reduction-oxidation and catalytic reactions to produce various corrosion films depending on its chemical environment. Near ambient pressure X-ray photoelectron spectroscopy, polarized modulated infrared reflection absorption spectroscopy, and Auger electron spectroscopy were used to study the key reactants, from O 2 (g), H 2 O vapor, Na + and Cl – on the initial stages of iron surface corrosion. Here, with increasing the ratio of O 2 and H 2 O, surface hydrocarbons were shown to oxidize into carbonates, while the Cl – was found to migrate into the interface. The effect of each individual reactant was measured separately and water was shown to have a first order rate dependence on the carbonate growth at low pressures, with little dependence for O 2 . Near ambient pressures, both H 2 O and O 2 were found to increase the carbonate growth, which was estimated using the Langmuir isotherm model, yielding Gibbs energies between –9.8 to –8.5 kJ/mol. A mechanism is suggested to explain the oxidation is catalyzed by NaCl on iron surfaces and the adventitious hydrocarbons served as the source for surface carbonation. These findings have implications for understanding other surface catalytic and redox interface chemistry in complex environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Pseudomonas aeruginosa Dps (PA0962) Functions in H 2 O 2 Mediated Oxidative Stress Defense and Exhibits In Vitro DNA Cleaving Activity

We report the structural, biochemical, and functional characterization of the product of gene PA0962 from Pseudomonas aeruginosa PAO1. The protein, termed Pa Dps, adopts the Dps subunit fold and oligomerizes into a nearly spherical 12-mer quaternary structure at pH 6.0 or in the presence of divalent cations at neutral pH and above. The 12-Mer Pa Dps contains two di-iron centers at the interface of each subunit dimer, coordinated by conserved His, Glu, and Asp residues. In vitro, the di-iron centers catalyze the oxidation of Fe 2+ utilizing H 2 O 2 (not O 2 ) as an oxidant, suggesting Pa Dps functions to aid P. aeruginosa to survive H 2 O 2 -mediated oxidative stress. In agreement, a P. aeruginosa Δdps mutant is significantly more susceptible to H 2 O 2 than the parent strain. The Pa Dps structure harbors a novel network of Tyr residues at the interface of each subunit dimer between the two di-iron centers, which captures radicals generated during Fe 2+ oxidation at the ferroxidase centers and forms di-tyrosine linkages, thus effectively trapping the radicals within the Dps shell. Surprisingly, incubating Pa Dps and DNA revealed unprecedented DNA cleaving activity that is independent of H 2 O 2 or O 2 but requires divalent cations and 12-mer Pa Dps.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2024

Accretion of the earliest inner Solar System planetesimals beyond the water snowline

How and where the first generation of inner Solar System planetesimals formed remains poorly understood. Potential formation regions are the silicate condensation line and water snowline of the solar protoplanetary disk. Whether the chemical compositions of these planetesimals align with accretion at the silicate condensation line (water-free and reduced) or water snowline (water-bearing and oxidized) is, however, unknown. Here we use the Fe/Ni and Fe/Co ratios of magmatic iron meteorites to quantify the oxidation states of the earliest planetesimals associated with non-carbonaceous (NC) and carbonaceous (CC) reservoirs, representing the inner and outer Solar System, respectively. Our results show that the earliest NC planetesimals contained substantial amounts of oxidized Fe in their mantles (3–19 wt% FeO). In turn, we argue that this required the accretion of water-bearing materials into these NC planetesimals. The presence of substantial quantities of moderately and highly volatile elements in their parent cores is also inconsistent with their accretion at the silicate condensation line and favours, instead, their formation at or beyond the water snowline. Similar oxidation states in the early formed parent bodies of NC iron meteorites and those of NC achondrites and chondrites with diverse accretion ages suggest that the formation of oxidized planetesimals from water-bearing materials was widespread in the early history of the inner Solar System.

Damanveer S. Grewal↗

DOE OSTI2025

Low-Temperature Processing of Pyrolysis Bio-Oil for Sustainable Biographite Production

Catalytic graphitization of pyrolysis bio-oil with iron (Fe) can produce an anode material for lithium-ion batteries (LIBs) at a moderate temperature. The key challenge to scaling up the process is foaming, which occurs due to the oxidation of Fe by the organic acids present in bio-oil. This study explored five different pathways to control foaming in bio-oil upon Fe addition, including (i) defoamers use, (ii) use of iron oxide (Fe2O3) as graphitization catalyst, (iii) pH adjustment of bio-oil, (iv) bio-oil coking (300-500 degrees C), and (v) low-temperature pretreatment of bio-oil (150-200 degrees C). The low-temperature pretreatment successfully avoided foaming by removing the volatile acids in bio-oil. The bio-oil was solidified and powdered for even mixing with the Fe catalyst. The biographite catalytically prepared at 1500 degrees C following this pathway demonstrated nearly theoretical specific gravimetric capacity (~370 mAh/g), high initial Coulombic efficiency (90.03%), and minimal capacity fading after 50 cycles in LIB half-cells. The low-temperature pretreatment pathway also addressed the viscosity, swelling, and aging issues associated with bio-oil processing and will make scale-up endeavors more attainable.

09 BIOMASS FUELS↗

NASA NTRS1999

Ceruloplasmin ferroxidase activity stimulates cellular iron uptake by a trivalent cation-specific transport mechanism

The balance required to maintain appropriate cellular and tissue iron levels has led to the evolution of multiple mechanisms to precisely regulate iron uptake from transferrin and low molecular weight iron chelates. A role for ceruloplasmin (Cp) in vertebrate iron metabolism is suggested by its potent ferroxidase activity catalyzing conversion of Fe2+ to Fe3+, by identification of yeast copper oxidases homologous to Cp that facilitate high affinity iron uptake, and by studies of "aceruloplasminemic" patients who have extensive iron deposits in multiple tissues. We have recently shown that Cp increases iron uptake by cultured HepG2 cells. In this report, we investigated the mechanism by which Cp stimulates cellular iron uptake. Cp stimulated the rate of non-transferrin 55Fe uptake by iron-deficient K562 cells by 2-3-fold, using a transferrin receptor-independent pathway. Induction of Cp-stimulated iron uptake by iron deficiency was blocked by actinomycin D and cycloheximide, consistent with a transcriptionally induced or regulated transporter. Cp-stimulated iron uptake was completely blocked by unlabeled Fe3+ and by other trivalent cations including Al3+, Ga3+, and Cr3+, but not by divalent cations. These results indicate that Cp utilizes a trivalent cation-specific transporter. Cp ferroxidase activity was required for iron uptake as shown by the ineffectiveness of two ferroxidase-deficient Cp preparations, copper-deficient Cp and thiomolybdate-treated Cp. We propose a model in which iron reduction and subsequent re-oxidation by Cp are essential for an iron uptake pathway with high ion specificity.

NASA Discipline Regulatory Physiology↗

NASA NTRS1989

Interfacial chemical reactions between MoS2 lubricants and bearing materials

XPS and conversion-electron Moessbauer spectroscopy (CEMS) were used to examine iron that was deposited on the basal plane of MoS2 single crystals and subjected to vacuum annealing, oxidizing, and reducing environments. Iron either intercalated into the MoS2 structure or formed oriented iron sulfides, depending on the level of excess S in the MoS2 structure. CEMS data demonstrated that iron sulfide crystal structures preferentially aligned with respect to the MoS2 basal plane, and that alignment (and potentially adhesion) could be varied by appropriate high-temperature annealing procedures.

Zabinski, J. S.↗

DOE OSTI2023

Inhibition of Extracellular Enzyme Activity by Reactive Oxygen Species upon Oxygenation of Reduced Iron-Bearing Minerals

The dual roles of minerals in inhibiting and prolonging extracellular enzyme activity in soils and sediments are governed by enzyme adsorption to mineral surface. Oxigenation of mineral-bound Fe(II) generates reactive oxygen species (ROS), yet it is unknown whether and how this process alters the activity and functional lifespan of extracellular enzymes. Here, the effect of mineral-bound Fe(II) oxidation on the hydrolytic activity of a cellulose-degrading enzyme ß-glucosidase (BG) was studied using two pre-reduced Fe-bearing clay minerals (nontronite and montmorillonite) and one pre-reduced iron oxide (magnetite) at pH 5 and 7. Under anoxic condition, BG adsorption to mineral surface decreased its activity but prolonged its lifespan. Under oxic condition, ROS was produced, with the amount of •OH, the most abundant ROS, being positively correlated with the extent of structural Fe(II) oxidation in reduced minerals. •OH decreased BG activity and shortened its lifespan via conformational change and structural decomposition of BG. These results suggest that under oxic condition the ROS-induced inhibitory role of Fe(II)-bearing minerals outweighed their adsorption-induced protective role in controlling enzyme activity. These results disclose a previously unknown mechanism of extracellular enzyme inactivation, which have pivotal implications for predicting the active enzyme pool in redox-oscillating environments.

58 GEOSCIENCES↗

NASA NTRS1993

A Moessbauer spectrometer for the mineralogical analysis of the Mars surface: First temperature dependent tests of the detector and drive system

Part of the scientific payload of the Mars-96 mission is a Fe-(57)Mossbauer (MB) spectrometer installed on a small rover to be placed on the surface of Mars. The instrument is under development at the University of Darmstadt. This instrument, with some modifications, is also included in the scientific payload of the proposed MARSNET mission of the European Space Agency (ESA). A similar instrument is currently under development in the US. The reason for developing a Mossbauer spectrometer for space applications is the high abundance of the element iron, especially on the surface of Mars. The elemental composition of Martian soil was determined during the Viking mission in 1976 but not it's mineralogical composition. One believes that it is composed mainly of iron-rich clay minerals, with an iron content of about 14 (plus or minus 2) wt-percent, partly magnetic. Of extremely great interest are the oxidation state of the iron, the magnetic phases and the mineral composition of the Mars surface. To these questions MB spectroscopy can provide important information, which are not available by other methods. We report on first tests of the experimental setup in the temperature range plus 20 C to -70 C, roughly corresponding to the temperature range on the surface of Mars. Also questions concerning the signal/noise ratio (S/N) are discussed.

Held, P.↗